Dimethylcarbamoyl Chloride → HCID 69748249, compound

HRID 2181613Notes

Reaction equation

HRID 2181613 reaction equation
[CH3:1][CH:2]1[CH2:7][NH:6][CH2:5][CH:4]([CH3:8])[NH:3]1.C(N(CC)CC)C.[CH3:16][N:17]([CH3:21])[C:18](Cl)=[O:19]>C(Cl)Cl>[CH3:16][N:17]([CH3:21])[C:18]([N:3]1[CH:4]([CH3:8])[CH2:5][NH:6][CH2:7][CH:2]1[CH3:1])=[O:19]

Participants

5

Reactant 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 660562,6-Dimethylpiperazine

Product 1

HCID 69748249HCID 69748249, compoundYield 70%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To an ice-cold solution of 2,6-dimethyl piperazine (179 mmol, 20.4 g), methylene chloride (200 mL), and triethylamine (214 mmol, 29.9 mL) was added dropwise dimethylcarbamoyl chloride (179 mmol, 16.4 mL). After 4 hr the reaction was quenched with a saturated sodium bicarbonate solution and the methylene chloride layer was collected, dried, filtered and the filtrate was evaporated to dryness to obtain an orange oil, 2,6-dimethyl-piperazine-1-carboxylic acid dimethylamide (70%, 23.1 g).

Workup

  1. customAfter 4 hr the reaction was quenched with a saturated sodium bicarbonate solution
  2. customthe methylene chloride layer was collected
  3. customdried
  4. filtrationfiltered
  5. customthe filtrate was evaporated to dryness

Sources & evidence

ORD record
ord-61765786640a449db6baee62d62d034a
Source dataset
uspto-grants-2005_05
Patent number
US06894047B2

Reaction notes

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